Process for drying wet carbon black pellets



July 22, 1958 T. s. wHlTsEL, JR 2,843,942

PROCESS FOR DRYING WET CARBON BLACK PELLETS Filed Deo. 7, 1953 2 Sheets-Sheet 1 N ZU) o O m0 N o 'Q c, ff a O N tr i: EDM l" JZ Z C u O U u l m Ld z Q L.; I f

t o Z 2 O N O u I jimi l 5t; I 2 3;. lk l INVENTOR. N T.S.WH|TSEL,JR. 2,C 32 OJ BY 25E; In' M4 U ATTORNEYS July 22, 1958 PRocEss Filed Deal 7, 1953 T. s. wHlTsEL., JR 2,843,942

FOR DRYING WET CARBON BLACK PELLETS 2 Sheets-Sheet 2 F IG. 2.

' IN V EN TOR.

T. S. WHITSELVJR A T TORNEKS United States Patent APROCESS FORHDRYING WETy CARBON :BLACK PEILILETS Travis S. Whitsel, Jr. Borger, Tex,.assignor to Phillips PetrleumlCompany, a corporation of Delaware ApplicationiDecember 7,1953,; Serial No.13965'503 .7. Claims. (Cl. 3.4-1.0)

"This 1 invention `relates to the dryingfof pelleted solids. In one aspect, itlrelatestofaproce-ss-forfdrying carbon blacks pelle-ts` produced by ta-wet -pelleting process. {inanotherfaspect, it -relatesto `a A,novel vcombina-tion of; process steps wherein -wetcarbon ublack pellets are dried, Yand Water and'carboneblack dust obtained in said-process yare recovered and recycledto l a wet'gpelleting operation.

It isiknown int-he -art tow'pellet"carbon'blacle ""Pelleted carbon blackhas the advantages, yascompared ,tounpelleted or loose lcarbon-black, of` being capable of being stored, `transported, or otherwise handled without the formationf large amounts of 'dust,.-,whic,h would result in loss and inconvenience.

Two general types ofpelletingprocesses.arewgenerally recognized in the art. 'One ofthese is" known as a `dry pelleting process, wherein a mass .of relatively dryunpelleted `carbon Ablack `is rolledfin, a lowfvelocity, rota-ting drum at a moderately ,elevated temperature; .and pelletsof the carbonlblack j form as a result `Vof `cornpressioin,ofthe loosecarbon 4black bytheverlying mass otcarbon black. A second ,method is` known as:.thewetpelletingmethod anfd comprises the formation Gtia slurryor. paste ,ofi loose carbon ,black with .a4 predetermi-ned..arnount jot water, and the `forming of this paste into ,the ipellets, by extrusion through ,a dieor, `agitation witha special typetofagitator, ollowedbydrying ofthe wet pellets. .'It;is:.with-,aiwet pelleting method that thepresent invention is chiefly. concerned.

'Generally stated,` the. present. invention` comprises maintaining a densetluidizedbed of-,wetipelleted solidnmaterial; passing, a `.dn/ing,aas upwards/through said 4bed-ata uidizing velocity, L.; e.,.fat.s,uchl a' velocity thatA hindered settlingoccurs; and .withdrawingdried :pellets from an upper portionof .saidibed 5Dried pellets faregpreferably removed from f `th,e.-lluidize,d` bed ata ilOQus remote -from thejlocus ,of introductiontof Wet pellets. It fhasslaeenl found that in a. tiuidizedtbed of, pellets; maintained under hindered `settling.,conditions, `wet; pelletsfgby virtueof.- their greater density, =igravit ate ptowardpa 1 lowernportionof .the u-idizedi be.'l,-wh ile;t.lried;pellets,; on account `of .thein 'lesser densitymov,e toward the Uppervportionrof :saidwbe'dand can be selectively withdrawn therefrom. The present invention isdistinguished fromrprocessesin which.the dry pelletingi of. .carbon 1. blackjs .etected: by thetiuidization of amass of; loose or; unpelleted carbon black, since in-suoh a ,process `a separationwof `dried :from-.twet `pelletsis not water which? is removed during thexlrying process; is condensedeand' recycledv to thecwetpelleting. operation. ",This

I 2,843,942 Patented July' 22', 1958 l2 water, which-has been evaporatedlfromthe 'carbon' black pellets, has substantially Athe characteriof "distilled water. It is substantially "free of mineralmatter-and, therefore, is rof -aY purity-highly ldesirable -in* a -wetg pelleting process, since Vit introduces substantially no ashLforrning material into the carbon `black pellets.

According to .anotheremodication of thejpresent invention, loose carbonblack-orcarbon black dust, which'is formed -inismallamounts as a result of `attrition of the. carborrfblaek` pellets during the `drying,.operation, is recovered together-with the water condensed'from'the used 'drying gas vand -is-Arecycled :with-the `recovered .water to the wet pelle-.ting operation, thus substantially reducing attrition losses.

According to Va further modilication lof theinvention, the depth of lthe tluidizedhedof: carbon blackpelletsjis controlled by controlling the; height or .level at which dried pellets are withdrawn from the flui'dzed bed. lSi nce, s, rn attrition occurs during `the dryingfitis Vdesirable notto extend, unduly, the residence time of appelletiin thedrying' zone. "The most desirable time .wilLdepend @P011 several factors, Vsuch as the initial water content ,ofthe wetp'ellets, the temperature dilerential between the Vinc;omirlg..andeutgoing Ydrying` gas, the moisture content ofjthedrying gas, and the'desired degree of d rying. JThus,.aCC'Qtditlg to4 this invention, the optimum4 residence` time of arpellet within the drying zone is readily obtained.

In the drawings, n

Figure 1 s Va diagrammatic `ow sheetjillusnatingone embodiment of this invention.

Figure 2 illustrates diagrammaticallyanother!embodiment of this invention. 4

-'Figure 33 illustrates diagrammatically ,stillY another .ennbodiment of the invention.

)Als illustrated L in Figure y1, loose, .nnpelleted `carbon black enters wet pelleting zone'4,tht0llgh,in1t.l. ,Aiptedetermined amountiof water., enterszoneA throughinlet. Wetpellet-ing zone y4 represents.,anywegpellotiuglprocess known in the art, and the relativeproportionsofiloose carbon black andwater introduced. .iuozonetarelcnown in the wet pe'lleting art.

'Pellets formed in zone `4 pass,` forexarnplghy, gravi-ty, through conduitS into. dryingizone f6, whichsordinaril-y a vertically elongated, ,generally cylindrical,eontginerpf desired capacity. 'l`hedryir 1gE gas. enters heating rzone 9 through inlet'10. Heatingzonecanbe of ,any/,suitable design known in 'the art for the heatiugof ages. ,The ,drying fgas` S Ordinarily belated. .t0 ,a temperature,aboveathe boiling point of waterunder the pressureofgdryingizone 6. Preferably, this temperature is ,in...the,range1 500-1to 1000 "E, however, temperatures. below., t,hisrran ge canfoe used.

,Suitable drying gases, are hydrogemgcarbon,monoxide, carbon r"dioxide7 nitrogen, methane, athene, naturalisas, residue gas, combustion or,v.uegas,.and air. Qf i these u, gases, carbon` dioxide and/ or nitrogen arefoftenipreferred because of theirnon-toxicitynd generalV cherncaliinertness. When air isused;as 4thedryingfgasna relatively,low`

of carbonblack .pellets `isgrnai-ntained 'mi tnnbugleuifidense phase which, .inf appearance, resembles; `a aboilngsliqild- 0 Thus, ,Substantially .all .ofthe carbonblacls remains within drying ,zone 6 and 4doesinotiptiss fr-Qlflisaid,zonenwithttlfiel ,vont-timing ,gas Conditions .of the .deseribediane generally known as hindered settling conditions. Under such conditions, a separation of solid particles subjected to the hindered settling conditions is obtained, based on differences in density of the solids subjected to such conditions. It has been found that the wet carbon black pellets, being of greater density than dried pellets, tend to settle toward the bottom of the uidized bed, while dried pellets are displaced upwardly toward the top of the bed. The dried pellets are withdrawn from the upper part of the bed through outlet 11, which can be in the form of a gravity stand-pipe which extends into the iluidized bed in drying zone 6 `and to the top, or almost to the top, of the upper level of the lluidized bed, designated as 7 in the drawing. The carbon black pellets are withdrawn from the iiuidized bed at a point laterally remote from that at which wet pellets are introduced and at a temperature preferably above the boiling point of water under the conditions of contacting. A preferred temperature of the withdrawn pellets is from about 250 to about 350 F. and, more desirably, about 300 F. The pressure within the drying Zone 6 is ordinarily about atmospheric or slightly super-atmospheric, e. g., 14 to 100 p. s. i. g. Vacuum operation is feasible, however. The withdrawn pellets are -cooled by any suitable means in cooling Zone 12, and dried pellets of carbon black are withdrawn as product through outlet 13.

The wet pellets supplied to drying zone 6 through inlet ordinarily contain from about 50 to about 57 weight percent water. Part of the sensible heat of the drying gas introduced through line 8 heats the pellets to a temperature Iat which the water diffuses to the surface of the pellets 'and vaporizes.

The used drying gas withdrawn from drying zone 6 through conduit 16 contains appreciable amounts of Water and small amounts of carbon black dust produced by attrition of the pellets during the fluidization in zone 6. Over a long period of time, the loss due to attrition and dust formation could be substantial. Therefore, according to one embodiment of lthis invention, the carbon black dust is recovered from the effluent drying gas. Furthermore, the water which has been removed by vaporization from the wet pellets in zone 6 is, for purposes of this invention, distilled water and is of purity suitable for reuse in the pellet'ing operation. Therefore, the gas which is Withdrawn through conduit 16 is subjected to cooling so that the water therein is condensed and recovered. Substantial proportions of carbon black dust are also recovered, together with the condensed water, and the dust recovery can be increased, if desired, by subjecting the gas to cooling and passing it through a conventional gassolids separation means, such as a mist precipitator or a cyclone separator. The recovered water is preferably recycled to the wet pelleting operation, together with the carbon black recovered along with the water, through conduit 18. However, the recovered material can be withdrawn from the system through outlet 19, if desired.

Drying gas, freed of Water and carbon black dust, is preferably recycled to heating zone 9 through conduit 20 but can be Withdrawn from the system, totally or in part, through outlet 23.

Alternatively, part of the gas withdrawn through conduit 16 can be directly recycled through conduits 21 :and 20 to heating zone 9, thus retaining part of the sensible heat remaining in the eflluent drying gas. Also, alternatively, the efluent drying gas can be exhausted to the atmosphere, totally or in part, through outlet 22.

It has been found desirable, on account of the high rate of heat transfer within the fluidized bed, to control automatically the temperature of the ingoing drying gas in accordance with the temperature of the eflluent gas. Thus, the temperature of the eliluent gas in conduit 16 can be measured by suitable temperature measuring means 14, and the temperature thereof can be converted to :any suitable form of energy to actuate control means 15, which, in turn, controls the heat supply within zone 9.

,4 Control means 15 can be any desired suitable combination of servo mechanisms, amplifiers, motor valves (e. g., controlling fuel gas supply) and similar devices known in the art.

According to Figure 2, the depth or level of the fluidized bed, and consequently the residence time of pellets in zone 6, can be Varied in accordance with particular requirements by the use of outlet conduit 11 in the form of a manifold having branch pipes 11A, 11B, and 11C, each of which is provided with a suitable valve means. Thus, by opening only conduit 11A, a bed level corresponding to 7 is obtained; whereas by opening conduit 11B, a bed level corresponding to 7A and a corresponding shorter residence time are obtained. Likewise, by opening conduit 11C, :a bed level corresponding to 7B and a still shorter residence time are obtained. Any suitable number of branched conduits can be used, `as needed.

As shown in Figure 3, the bed level 7 can be adjusted by the use of a vertically moveable outlet 11, which is provided with a suitable sealing means or packing gland 25. Thus, the height of outlet 11 can be adjusted to any desired level to obtain any desired residence time.

It has been customary in the prior art to dry wet carbon black pellets by passing them through an externally,

(3) Increased heat economy-Heat transfer rates in.

a uidized bed are extremely high, primarily because of the large surface area of the bed of particles. Thus, the efluent drying gas is ordinarily at substantially the same temperature as the iluidized bed at a given point.

(4) Increased efficiency of control-In the prior art, the amount of fuel supplied to the burners of a rotary dryer has been controlled in accordance with the temperature of the dried pellets. In such a separation, there is a substantial time lag caused by low heat transfer rates in a rotary dryer. The present invention facilitates control by regulating the inlet temperature of the drying gas in accordance with the outlet temperature of the used gas. Thus, there is substantially no time lag in the control, according to the present invention.

Although certain process steps, structures, and examples have been described for purposes of illustration, it is clear that the invention is not limited thereto; for example', the present invention is applicable to the drying of catalyst orabsorbent pellets, as well as carbon black pellets. Also, wet pellets can be introduced into an intermediate or lower level in the fluidized bed, e. g., in suspension in the drying gas. From the foregoing, it will be evident that the essence of this invention is that wet pellets are dried by introduction into a fluidized pellet bed, passing a drying gas upwardly through said bed, and selectively removing dried pellets from an upper portion of said iluidized bed.

I claim:

l. A process which comprises forming wet pellets of carbon black by a wet pelleting method, introducing said wet pellets into an upper part of a bed of carbon black pellets maintained under hindered settling conditions 4in an yobstructed drying zone by the passage of a hot drying gas upwardly therethrough; heating said drying gas, prior to contacting with said bed, to supply all of the heat required to raise the temperature of said -bed above the boiling point of water under the conditions of contacting, whereby water is vaporized and removed from the pellets and dried pellets are caused to move to an upper portion and wet pellets to a lower portion of said bed; and withdrawing dried pellets from a locus, in an upper part of said bed, remote from that at Which wet pellets are introduced, said dried pellets being withdrawn at a tempera- V ture above the boiling point of water; withdrawing used 5 drying gas from said bed; and cooling and recovering said dried pellets.

2. A process according to claim 1, wherein water is recovered from said used drying gas and recycled for use in said wet pelleting method.

3. A process according to claim 2, wherein carbon black dust is recovered and recycled together with said water.

4. A process for drying wet pellets compacted from particulate solid material comprising introducing said pellets into an unobstructed drying zone countercurrently to a hot drying and fluidizing gas introduced to a lower section of said zone; passing said hot gas thru said zone at a iluidizing velocity to maintain a dense iluidized mass of pellets so as to heat and dry same, said hot gas being the sole means of heating and drying said pellets; gravitating dried pellets from an upper section of the iluidized mass of pellets in said zone; and withdrawing eluent gas from a section of said zone above the pellet introduction and removal levels.

5. A process according to claim 4, wherein said Wet pellets contain from 50 to 57 per cent water.

6. A process according to claim 4, wherein said drying gas is introduced into said bed at a temperature in the 6 range 500 to 1000 F. and said dried pellets are withdrawn at a temperature of about 300 F.

7. A process according to claim 4, wherein said wet pellets are introduced into said bed at an upper level therein and at a locus remote from that at which said dried pellets are withdrawn.

References Cited in the file of this patent UNITED STATES PATENTS OTHER REFERENCES Industrial and Engineering Chemistry, voll. 41, No. 6, June 1949, Fluid-Solid Air Sizer and Dryer, pages 1247 to 1249, 34-57.

UNITED STATES PATENT OFFICE CERTIFICATE OF CORRECTION Patent No. ,29843,942 July 22, 1958 Travis S Whitsel, Jr.

It is hereby certified that error appears in the printed specification of tlde above numbered patent requiring correction and that the said Letters Patent should read as corrected below.

Column 4, line 52, for "absorbent" read fc-1 adsorbent line 65, for Hobstructed" read unobstructed Signed and sealed this 24th day of February 1959.,

(SEAL) Attest:

KARL H. MINE Attesting Officer ROBERT C. WATSON Commissioner of Patents 

